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  • 1
    ISSN: 0044-2313
    Keywords: Titanium-Aluminium Alkoxide ; Aluminium Titanate (Tialite) ; Ceramics Precursor ; X-Ray Structure Determination ; 1H/13C-NMR (2 D) ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Description / Table of Contents: Synthesis and Structural Characterization of a Novel Titanium-Aluminium AlkoxideThe novel Ti-Al-Alkoxide TiAl2(OiPr)10, was synthesized from aluminium turnings and titanium tetraisopropoxide in 2-propanol and isolated by subsequent fractionating distillation. Colourless prismatic crystals precipitated after 24 h at 20°C from the main fraction. They proved very moisture sensitive. The compound crystallizes in the monoclinc space group C2/c (no. 15) with a = 2303.1(4), b = 1097.2(3), c = 1685.0(3) pm, β = 104.32(1)° and Z = 4. The molecular structure exhibits a bent Al-Ti-Al′ unit, in which Al shows tetrahedral, but Ti octahedral1 coordination. The polyhedra are connected via cis-edges of the octahedron. The structure of the compound in solution was determined by NMR spectroscopy (1H, 13C, COSY) and proved to be identical to the structure in the solid state.
    Notes: Das neue Ti-Al-Alkoxid TiAl2(OiPr)10 wurde durch Umsetzung von Al-Spänen mit Titantetraisopropoxid in Isopropanol und anschließender fraktionierender Destillation dargestellt. Die nach 24 h bei 20°C aus der Hauptfraktion gebildeten farblosen, prismatischen Kristalle sind sehr hydrolyseempfindlich. Die Kristallstruktur konnte bei -83°C bestimmt werden: monokline Raumgruppe C2/c (Nr. 15) mit a = 2303,1(4), b = 1097,2(3), c = 1685,0(3) pm, β = 104,32(1)° und Z = 4. Die Molekülstruktur besteht aus einer gewinkelten Al-Ti-Al′-Einheit, in der Al tetraedrisch und Ti oktaedrisch koordiniert sind. Die verknüpfenden Kanten am Ti-Oktaeder sind cis angeordnet. Die Struktur der Verbindung in Lösung wurde NMR-spektroskopisch (1H, 13C, COSY) ermittelt und stimmt mit der Struktur im Einkristall überein.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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  • 2
    ISSN: 0009-2940
    Keywords: Diaminosulfanes / Disilanes / Sulfur diimides ; Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: A New Route to N-Silylated Diaminosulfanes: The Splitting of the Si — Si Bond in Disilanes by Sulfur DiimidesSulfur diimides (R1N)S(N2) (R1, R2 = tBu, SiMe3; 1a-c) and disilanes Cl2(R)Si-Si(R)Cl2 [R = Me (2), Cl (3)] react fast and quantitatively in a 1:1 ratio to give diaminosulfanes (4, 5) by cleavage of the Si-Si bond. The solid-state structure of tBu(SiMeCl2)N-S-N(SiMe3)SiMeCl2 (4b) has been studied both by X-ray crystallography and 29Si-NMR spectroscopy.
    Additional Material: 1 Ill.
    Type of Medium: Electronic Resource
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